Production of molecular compounds



Patented ay 10, use

'rso, STATES,

a; [rice 2,118,640 PRQDUCTION OF MOLECULAR COMPOUNDS, Kurt Quehl. Zwickau, Germany, assignor to Chemische Fabrik many Theod. Rotta, Zwickau, Ger- 'No Drawing. Application February 24, 1936, Se-

rial No. 65,432. In Germany February 2'1,

. ing such molecular compounds, and to textiles disclosed by the components as such and of a na-- treated therewith.

It' has been proposed already to use ureasfor purposes of thetextile industry. For example,

British Patent No. 251,993 discloses the emp y-'- ment thereof for finishing. British Patent No. 285,992- and French Patent N0. 653,658 descr b the use of urea as a swelling'agent for artificial silk, particularly acetate silk, and British Patent Nos. 318,978; 318,469 and 262,830 recommend additions of ureato dye-baths.

According to these disclosures, ureacan be used also in the presence of other compounds, and on examination it will be found that such other substances are to be added in quantities not narrowly proportionateto the urea used. They constitute therefore pure mixtures, and it was iustiflable to expect that they would disclose merely the properties of their various components.

American Patent No. 1,979,121 showed, however, that molecular compounds of urea and inorganic or organic salts possess properties not ture to render these compounds'excellently suitable for finishing purposes. The urea and 'salt compounds of the general formula rmewomrnnmx.

It is further known to employ in the textile industry sugar of various kinds, such as grape sugar, cane sugar, 8130., for imparting tofabrics greater stiffness and more feel. Sugar, however, can be used only within relatively narrow limits, because if applied in larger amounts to the fiber the colors of the textiles will often appear lightly covered thereby and the sugar may come -off. in dust-dike particles. Furthermore, this leading with sugar frequently imparts to the fabric an unpleasant sticky feel and causes its rejection by users;

. 13 Claims. (Cl. 260-10) According to'the invention, these drawbacks can be avoided by employing molecular compounds 01' urea and saccharoses.

These molecular compounds of urea and a mono-, dior poly-saccharose represent new chemical compounds having a uniform relatively sharp melting point. Like most molecular compounds they possess the chemical properties of their components, but disclose .a considerably different physical'behavior. Theirsolubility conditions in particular are different, as they usually dissolve more easily in water and crystallize much more difiicultly. A remarkable feature of compounds irom such solutions is their low adhesive power. 7

Compounds of this class can be obtained in a simp.e manner by dissolving the components in each other and'heating to liquefaction, i. e., by

.fusing urea in eq imolecular or double equimolecular quantity with. respect to the saccharose, or

by evaporating a solution of both in'a suitable solvent like water, methyl alcohol, etc. on the water bath and heating the residue up to melting. In most cases the temperature of the water bath will be sumcient, though higher temperatures may be useful, especially to insure rapid conversion of the components. According to the kind of saccharoses employed, the time required for conversion differs slightly, though those skilled in the art will have no difflculty in iinding out when; the conversion is completed.

S accharoses practically suitable for conversion with urea on account of being available in suiiicient quantities are for instance 4- and 5-hydroxyl aldehydes and ketonic alcohols like arablnose, glucose, .galactose, levulose as monosaccharides. Of the di-saccharoses, cane-sugar, lactose and maltose may be mentioned; and of the polysaccharoses, ramnose. Mixtures of these can of course be used also.

These molecular compounds crystallize so difficultlythat crystallization can be brought about only by resorting to measures like precipitating with alcohol, rubbing with a glass rod and inoculating theiused mass when cold with asmall .crystal. Identification was effected by the inventor in crystallized material only.

This low crystalline force renders such molecular compounds particularly suitable for finishing purposes, and finishing agents comprising them,

are therefore of great practical importance.

Whilst ithas frequently been observed that thev all tioned is not open to the same objection. It is even possible to load the textiles with larger quantities without causing efllorescence. Furthermore, since the application of agents comprising such molecular compounds makes: it possible to avoid the viscosity of sugar preparations, stickiness cannot appear at all or only to a very slight degree, even in case of high concentrations on the I fiber in typical weighting finishes. Compared with other agents like glycerin, the compounds described are less hydrophilic, whiclris highly desirable, as a fiber loaded for instance with to 20% glycerin, etc. from treating agents discloses such differences in weight depending on atmos-" pheric moisture that trading in such goods and finishing additions and--agents of. a diflerent or It is therefore possible to employ similar (type. them in the presence of glue, gelatin, starch, mucilages,' etc., and even sensitive softening" agents do not produce a reaction with the highly indifierent molecular compounds. Many different a combination effects can thus be obtained, which is of considerable importance in the finishing of textiles. i

' crystallize. Only-when the syrup is left standing.

The following examples are intendedto explain the nature of the invention without limiting it to the disclosures made therein..

Example 1 .The molecular compound of urea and glucose is obtainedby fusing 60 parts.by weight of urea with 198 p. b. w. 'of finely pulverized dry glucose at water bath temperature. Thesyrup obtained in about one hour normally does not tend to for some time and subjected to occasional'rubbing with a glass rod, small needles will separate therefrom, whereupon the largest portion poi the mass soon solidifies from the center' of crystallization and forms a crystal-magna. For identification application to clay is prferable. The

isolated little needlesmelt at 117 Cfafter drying on calcium chloride; glucose is known ,to melt at 85 C. and ur a at 132 C. The relatively sharp melting point s characteristic of the molecular compound. 7,

I v Example 2 y Viscose silk on the reel is treated with aliquor containing in 100 liters of water 10 kg. of a molecular compound according to Example 1, whereupon the goods are hydro-extracted and dried as usual. Material thus finished discloses an ex- .cellent feel, and its stability as to weight is good.

Example 3 Pure wool gaberdine is passed on-the padding machine through a liquor containing 3% of ordinary commercial parafiimand of a single bath impregnating agent containing alumina, to which furthermore of a molecular compound of 1 mol. of urea plus 1 mol. of cane-sugar has been both components in ;point.

added. The after-treatment of the goods is as usual. The finished material has a full feel, sheds water well and after treatment increases 12% in weight.

' Example 4 v The rear side of fancy cotton goods is treated with a finishing. liquor containing in 100' parts of water 5 parts by weight of soluble starch and p. b. w. of a molecular compound of 1 mol. of'

urea and 1 mol. of glucose by spraying. The remainder of the treatment is the usual one. The material obtained is highly weighted, but does not feel sticky, and even at considerable differences in atmospheric .moisture fluctuates in weight only withinpermis'sible limits. g

Iclaim:-' I p 1. As a new composition of matter the-molecularv compound, containing carbamide and saccharoses as components in molecular proportion up to 2:1, and disclosing the chemical properties of the said'components, but having lower crystalline force than each of said components and less adhesive power than. sugar in the form of more highly concentratedsolutions. "2. As anew composition of matter the mo-.

lecular compound of 1 molecule carbamide and one molecule glucose, said compound melting at 3. The process consisting in dissolving molecular quantities of urea and of saccharoses into one another in molecular proportions up to 2:1 while heating up to liquefaction.

4. The; process of producing novel molecular compoundaconsisting in dissolving urea and glucose in molecular quantities up to a 2: 1 ratio into one another at water bath temperature.

5. The process of producing novel molecular compounds, consisting in dissolving urea and saccharoses in molecular quantities up to a 2:1 ratio into one another in the presence of a solvent.

6. The process of producing novel tnolecular compounds, consisting indissolving urea and saccharoses in molecular quantities up to a 2:1 ratiointo one another by evaporation of a comthe water bath.

'7. As finishing agents fortextiles, comprisingmolecular compounds of carbamide and saccha- 8. A molecular compound of carbamide and saccharose components containing up to 2 molecular parts of the former component to one of the latter, exhibiting the chemical properties of said components, butsharply distinguished from respect to a fixed melting '9. A molecular compound of carbamide and s'accharose components containing up to 2 molecular parts of the former component to one of the latter, exhibiting the chemical properties oi said components, but distinguished from the latter component by a low property ofadhesion.

10. .A molecular compound of carbamide and saccharose components. containing up to -2molecular parts of the former component to one ofthe latter, exhibiting the chemical properties of said components, but distinguished from both] components in respect to sluggishness in-crystallization, i. e. crystallization takes place only, when started by introduction of a foreign agent.

11. A-molecular compound of carbamide and mon aqueous solution and heating the residue on,

the latter, exhibiting the chemical properties}! said components, but distinguished from both components in respect to ready solubility and a high capacity of being over-saturated in solution. 12. A molecular compound of carbamide' and saceharose components containing up to 2 molecular parts of the former component to one of KURT um. 

